Sugar-cane wax production



Patented Dec. 6, 1949 UNITED STATES PATENT 'OFFICE' 2.490.722 SUGAR-CANE wax rnonuc'rron Edward A. Wilder, Racine, Wis., assignor to s. 0. Johnson & Son, Inc., Racine, Wis.

No Drawing. Application July 12, 1946, Serial No. 683,139

12 Claims. (Cl. 260428.5)

but one of the most effective is described in U. S.

Patent No. 2,381,420 to Balch. By this method chipped or broken crude wax pieces are placed in a container and covered with a fat solvent, such as acetone, and the fatty portions are separated from the crude wax by a process of diffusing into the solvent. The disadvantage of this process, however, is that the diffusion takes a day, and is preferably repeated from three to seven times. From a commercial standpoint'the process is therefore ineflicient and would be costly, because of the length of time needed to carry out the process.

Now, in accordance with my invention, I have developed a method of obtaining hard wax from the crude sugar cane wax wherein the separation is carried out in a very few minutes, rather than in a matter of days. My method comprises heating the crude sugar cane wax until the wax is molten, then adding the molten wax to a fat solvent, such as acetone or methylethylketone, while the solvent is being maintained at a temperature below about 35 C., and preferably within the range of from about C. to about 25C., and agitating the solvent while the molten wax is being added. The hard wax is then recovered,

for example, by filtration. If desired, the pouring quality of the molten crude sugar cane wax may be improved by adding a small quantity of a single ring coal tar hydrocarbon, such as toulene,

- to the crude sugar cane wax.

Now, having indicated in a general way, the

nature and purpose of this invention, the folgiven in parts by weight, unless otherwise inin a vessel and heated to a temperature of about 85 C. until the wax was melted. Sixteen parts of acetone were placed in a cylindrical kettle 12" in diameter, 13" in depth, having a dished bottom. The kettle was provided with a water jacket for cooling. The temperature of the acetone was maintained within the range of 15 C. to 21 C. The solvent was agitated by a mixer of 1725 R. P. M. equipped with a 3" diameter, 3 blade propeller; which was set off center in order to create greater turbulence. After the agitation was started, the molten wax was poured into the solvent in a stream of about A," diameter. After the molten wax had been added to the solvent, agitation was continued for about '15 minutes, while the temperature of the solvent was maintained within the range of 15 C. to 21 C. The agitation was then discontinued and the waxsolvent mixture filtered. A substantial yield of hard wax was thereby recovered.

Example 2 Example 1 was repeated except that part of toluene was added to the crude sugar cane wax prior to melting. The addition of the toluene improved the pouring qualities of the molten wax.

Example 3 Example 2 was .repeated except. that benzene was substituted for toluene. This material was equivalent to toluene in improving the pouring qualitiesof, the molten wax.

Example 4 It is essential that the crude sugar cane wax 7 be heated until it is melted. While generally a temperature of C. to C. is suflicient, higher temperatures may be used. The use of higher temperatures, however, requires that more care be used to avoid darkening of the crude wax, and the heat transfer equipment must be adequate to handle the heat when the molten wax is introduced into the solvent.

. ing temperature A ratio of 16 parts of solvent to 8 parts (I wax is preferable, but, if desired. a ratio within the saidsolvent whilethemoltenwaxisbeingadded,

range of 2 parts of solvent to 1 part of crude wax to 4 parts of solvent to 1 part of crude wax may be used. If a greater concentration of solvent is used. a small percentage of hard wax will be lost in the soluble portion; while i! a lesser concentration of solvent is used, the concentration of the soft fraction may be so great that the separation of the hard wax fraction may be more dimcult.

The temperature of the solvent throughout the addition of the molten wax and during the agitavtion should be maintained at not more than 35 C. A temperature within the range of from about 10 C. to 25 C. has been found preferable; Temperatures below 10 C. may be used. but the solubility of the soft fraction decreases. Temperatures about 35 C. may be used, but carries some of the hard fraction into solution.

Although in the examples a water-jacketed vessel has been used to maintain the temperature of the solvent within the desired range, other well-known methods of heat exchange may be used to accomplish this purpose. However, if desired, no cooling is necessary provided the quantity of molten wax and the rate of addition does not raise the temperature of the solvent to more than 35 C.

While in the examples specific directions have been given as to the rate of introducing the wax into the solvent, speed of agitation, propeller d1? mensions, etc, it will be understood that these directions are'by way ofillustration only as they may be varied with the change in size of .equipment, ratio of wax to solvent, etc. Generally speaking, however, excellent agitation is required and any Of the well-known methods of obtaining good turbulence may be used. It is suggested that the agitator be set of! center, or a' vessel used with vanes, etc. to assist in getting greater turbulence.

There is no definite period that the agitation must be continued after the molten wax has been added to the solvent. As soon as the wax has been added the separation is substantially com-- pleted. In practice, however, it has been found advisable to continue the agitation for a period up to minutes after the wax has been added.

The addition of a single ring coal tar hydrocarbon, such as toluene, benzene or xylene, to the I crude sugar cane waxin the ratio oi not more than 1 part of hydrocarbon to 15 parts of crude wax by weight, is not essential. However, it improves fluidity and allows a slightly lower pourthan the use of molten wax alone.

After the agitation has been completed, the hard wax fraction can be recovered from the solvent by filtration, by centrifuging, or other knownmethods of separating the precipitate from the soluble portion.

Thus, by he process of my invention, I have succeeded reducing the time required for separating the hard wax fraction from the soluble from the group consisting of. acetone, methyb ethylketone, ethyl ether, heptane, hexane and pentane while maintaining the temperature of and recovering the hard wax fraction.

2. The method of obtaining a hard wax fraction from crude sugar cane wax comprising heating crudesugarcanewaxwithasingleringcoaltar hydrocarbon selected fromthe group consistin of benzene, toluene and xylene in the ratio of-not less than 15: 1 by weight until the mixture is fluid,

adding the hot mixture to a fat solvent selected from the/group consisting of acetone, methylethylketone, ethyl ether, heptane, hexane and pentane while maintaining the temperature of said solvent at not more than 35 0., agitating said solvent while the molten wax is being added and recovering the hard wax fraction.

3. The method of obtaining a hard wax fraction from crude sugar cane wax comprising heating crude sugar cane wax until the wax is melted, adding the molten wax to acetone while maintaining the temperature of said acetone at not more than 35 0., agitating said acetone while the molten wax is being added and recovering the hard wax fraction.

4. The method of obtaining a hard wax fraction from crude sugar cane wax comprising heating crude sugar cane wax until the wax is melted,

adding the molten wax to methylethylketone maintaining the temperature of said acetone within the range from about 10 C. to about 25 C.. agitating said acetone while the molten wax is being added and recovering the hard wax fraction.

6. The method of obtaining a hard wax fraction from crude sugar cane wax comprising heatingcrude sugar cane wax until thewaxismelted. adding the molten wax to methylethylketone while maintaining the temperature of said fmethylethylketone within the range from about 10- C. to about 25 C., agitating said methylethylketone while the molten wax is being added and recovering the hard wax fraction.

' 7, The method of obtaining a hard wax fraction from crude sugar cane wax comprising heating crude sugar cane wax anda single ring coal tar hydrocarbonselected from the group consisting of benzene, toluene and xylene in the ratio of not ,less than 15:1 by weight until the mixture is 25 C., said acetone while the molten fluid, adding the hot mixture to acetone while maintaining the temperature of said acetone within the rangeoi' from about 10 C. to about wax is being added and recovering the hard wax fraction.

8. The method of obtaining a hard wax fraction from crude sugar cane wax comprising heating crude sugar cane wax "and a single ring coal tar hydrocarbon selected fromthe group consisting of benzene, toluene-and xylene in the ratio of not less than- 15:1 by weight until the mixture is fluid, adding the hot mixture to methylethylketone while maintaining-the temperature of said methylethylketone within the range of from about 10. C.--to-about 259C. agitating said methylethylketone while the molten wax is being added and recovering the hard wax fraction. 1

9. The method of obtaining a hard wax fraction from crude sugar cane wax comprising heating crude sugar cane wax and toluene in the ratio of not less than 15:1 by weight until the wax is melted, adding the molten wax to acetone while maintaining the temperature of said acetone within the range of from about 10 C. to about 25 C., agitating said acetone while the molten wax is being added and recovering the hard wax fraction.

10. The method of obtaining a hard wax fraction from crude sugar cane wax comprising heating crude sugar cane wax and toluene in the ratio of not less than 15:1 by weight until the wax is melted, adding the molten wax to methylethylketone while maintaining the temperature of said methylethylketone within the range of from about 10 C. to about 25 C., agitating said methylethylketone while the molten wax is being added and recovering the hard wax fraction.

11. In a process of separating crude sugar cane wax into various constituents wherein crude sugar cane wax is treated with acetone, the improved steps comprising adding molten crude sugar cane wax to the acetone while said acetone is being maintained at a temperature of not more than 35 C. and agitating the acetone while the molten wax is being added.

EDWARD A. WILDER.

REFERENCES CITED The following references are of record in the file of this patent:

UNITED STATES PATENTS Number Name Date 1,808,755 Baylis June 9, 1931 2,145,784 Anderson Jan. 31, 19,39

2,270,214 Adams Jan. 13,1942 2,381,420 Balch Aug. 7, 1945 FOREIGN PATENTS Number Country Date 8,588 Great Britain of 1903 

